반응 #162994

반응 방정식

Potassium carbonate

hydroxylamine hydrochloride

4-nitrobenzonitrile

→

title product

수율 86.9%

N′-hydroxy-4-nitrobenzimidamide

수율 86.9%

용매

EtOAc

반응 조건

후처리

1. 1
   기타After completion of the reaction the solvent
2. 2
   기타was evaporated
3. 3
   기타the crude so obtained
4. 4
   세척washed with water, brine
5. 5
   건조dried by sodium sulfate
6. 6
   농축concentrated
7. 7
   기타to give a solid
8. 8
   기타purified by column chromatography
9. 9
   기타further recrystallized from EtOAc

실험 절차

Potassium carbonate and hydroxylamine hydrochloride were added to an ethanolic solution of 4-nitrobenzonitrile. The solution was refluxed at 80° C. for 5 hours. After completion of the reaction the solvent was evaporated and the crude so obtained was dissolved in EtOAc and washed with water, brine, then dried by sodium sulfate and concentrated to give a solid. It was the purified by column chromatography and further recrystallized from EtOAc: petroleum ether to obtain the title product in 86.88% yield. 1H NMR (DMSO-d6) δ: 6.071 (s, 2H, NH2) 8.24 (d, 2H, CH), 8.317 (d, 2H, CH), 10.138 (S, 1H, OH), ms (m/z) 180 (M−−H).

출처